Department of Chemistry, University of Ioannina, 45110, Ioannina, Greece.
University Research Center of Ioannina (URCI), Institute of Environment and Sustainable Development, 45110, Ioannina, Greece.
Anal Bioanal Chem. 2021 Nov;413(28):7129-7140. doi: 10.1007/s00216-021-03684-y. Epub 2021 Oct 1.
In recent years, the occurrence, fate, and adverse effects of pharmaceutically active compounds (PhACs) in aquatic organisms have become a noteworthy issue. In the present study, a rapid and sensitive multiresidue analytical method was developed for the determination of 18 parent PhACs and 5 metabolites in sea bream (Sparus aurata), by combining a modified QuEChERS (quick, easy, cheap, effective, rugged and safe) procedure with ultra-high performance liquid chromatography-Orbitrap-mass spectrometry (UHPLC-Orbitrap-MS). The method development involved optimization of extraction solvent, extraction salts, clean-up sorbents, and amount of sample evaluation, while identification on Orbitrap MS was based on accurate mass and further confirmation with MS/MS fragmentation. The developed method was validated, and linearity was higher than 0.99. Recoveries in all cases ranged between 62 and 107% (at 10, 50, and 100 ng g), while intra-day and inter-day precision, expressed as relative standard deviation, RSD, was lower than 4% and 7%, respectively. In addition, limits of quantification (LOQs) ranged between 0.5 and 19 ng g. The compounds presented a low matrix effect, between - 13 and 4%, while the expanded uncertainty U% estimated at the three spiking levels 10, 50, and 100 ng g was found below 49% in all cases. Finally, the validated method was applied to sea bream samples from an aquaculture farm located in the Mediterranean Sea, with one positive finding for the antibiotic trimethoprim at a concentration of 26 ng g, presenting negligible human health risk.
近年来，水生生物中药物活性化合物（PhACs）的出现、命运和不良影响已成为一个值得关注的问题。在本研究中，结合改良的 QuEChERS（快速、简便、廉价、有效、耐用和安全）程序和超高效液相色谱-轨道阱质谱（UHPLC-Orbitrap-MS），开发了一种用于测定海鲈（Sparus aurata）中 18 种母体 PhACs 和 5 种代谢物的快速灵敏多残留分析方法。方法开发涉及萃取溶剂、萃取盐、净化吸附剂和样品评价量的优化，而轨道阱 MS 上的鉴定则基于准确质量，并进一步通过 MS/MS 碎片进行确认。所开发的方法经过验证，线性度高于 0.99。在所有情况下，回收率均在 62%至 107%之间（在 10、50 和 100ng/g 时），而日内和日间精密度（以相对标准偏差 RSD 表示）分别低于 4%和 7%。此外，定量限（LOQs）范围在 0.5 至 19ng/g 之间。这些化合物的基质效应较低，在-13%至 4%之间，而在三个加标水平 10、50 和 100ng/g 下估计的扩展不确定度 U%在所有情况下均低于 49%。最后，该验证方法应用于位于地中海的一个水产养殖场的海鲈样本，在一个样本中发现抗生素甲氧苄啶的浓度为 26ng/g，呈现出可忽略的人类健康风险。
